反应详情

A mixture of α-methylbenzylamine (10.7 g, 0.088 mol), paraformaldehyde (21.1 g, 0.703 mol), acetic acid (10.2 mL, 0.179 mol) and 1-benzyl-4-piperidone (16.7 g, 0.088 mol) in MeOH (418 mL) was heated at reflux overnight. Upon cooling to room temperature the solvents were removed in vacuo. Water (700 mL) and KOH pellets (11.7 g, 0.209 mol) were added and the mixture was extracted with 3×150 mL CH2Cl2. The organic layer was dried (K2CO3), filtered and the solvent was removed in vacuo. The yellow residues were triturated with hexane and the combined organic solvents were concentrated to provide bispidine (1) as a crude yellow oil (26.7 g, 90%).

1. temperaturewas heated
2. temperatureat reflux overnight
3. customwere removed in vacuo
4. additionWater (700 mL) and KOH pellets (11.7 g, 0.209 mol) were added
5. extractionthe mixture was extracted with 3×150 mL CH2Cl2
6. dry with materialThe organic layer was dried (K2CO3)
7. filtrationfiltered
8. customthe solvent was removed in vacuo
9. customThe yellow residues were triturated with hexane
10. concentrationthe combined organic solvents were concentrated